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WO1994017243A1 - Adjuvants de retention pour les pates mecaniques - Google Patents

Adjuvants de retention pour les pates mecaniques Download PDF

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Publication number
WO1994017243A1
WO1994017243A1 PCT/CA1994/000021 CA9400021W WO9417243A1 WO 1994017243 A1 WO1994017243 A1 WO 1994017243A1 CA 9400021 W CA9400021 W CA 9400021W WO 9417243 A1 WO9417243 A1 WO 9417243A1
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WO
WIPO (PCT)
Prior art keywords
molecular weight
poly
composition
water
polyacrylamide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CA1994/000021
Other languages
English (en)
Inventor
Robert Pelton
Archie E. Hamielec
Huining Xiao
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dorset Industrial Chemicals Ltd
Original Assignee
Dorset Industrial Chemicals Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dorset Industrial Chemicals Ltd filed Critical Dorset Industrial Chemicals Ltd
Priority to EP94904545A priority Critical patent/EP0680532A1/fr
Priority to JP6516508A priority patent/JPH08504900A/ja
Priority to FI953468A priority patent/FI953468L/fi
Publication of WO1994017243A1 publication Critical patent/WO1994017243A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/36—Polyalkenyalcohols; Polyalkenylethers; Polyalkenylesters
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
    • D21H17/375—Poly(meth)acrylamide
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/47—Condensation polymers of aldehydes or ketones
    • D21H17/48—Condensation polymers of aldehydes or ketones with phenols
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/06—Paper forming aids
    • D21H21/10—Retention agents or drainage improvers

Definitions

  • the present invention relates to the provision of certain novel retention aids for mechanical pulps.
  • wood pulp comprising a highly dilute dispersion of wood fibers is placed onto a forming wire on which liquid is drained from the fibers to form a fibrous mat which then is processed further to form a paper sheet.
  • useful particulate components of the pulp such as fines, fillers and pigments, tend to pass out of the sheet and to be lost from the sheet into the filtrate.
  • SUBSTITUTE SHEET ions dictates that solutions be freshly-prepared on site at the pulp mill.
  • the present invention provides a novel chemical retention aid for mechanical pulps which both is effective in achieving retention of fines and yet does not suffer the drawbacks of the prior art.
  • the compounds utilized herein can achieve at least the same efficiency of fines retention in mechanical pulps as conventional high molecular weight polyoxyethylenes, but are stable and do not degrade as the prior art molecules do.
  • Such retention aid comprises a water soluble copolymer having a molecular weight of at least about 100,000 and comprising a high molecular weight water-soluble polymer backbone having pendant poly(oxyalkylene) groups.
  • a retention aid composition for use in the formation of a paper sheet from wood pulp, particularly mechanical pulp, comprising: (a) a water soluble copolymer having a molecular weight of at least about 100,000 and comprising a high molecular water-soluble polymer backbone having pendant poly(oxyalkylene) groups, and (b) a phenolic compound.
  • a slurry of cellulosic fibrous material, particularly mechanical wood fibers is dewatered and a retention aid composition is added to the slurry to improve the retention of fines, fibers and pigments in the paper sheet during the dewatering step.
  • the improvement comprises utilizing, as a component of the retention aid composition, a water-soluble copolymer having a molecular weight of at least about 100,000 and comprising a high molecular weight water-soluble polymer backbone having pendant poly(oxyalkylene) groups.
  • the copolymer employed herein may be formed from polymeric materials by grafting, preferably using radiation. Accordingly, in a further aspect of the invention, there is provided a method of forming a copolymer which comprises grafting pendant groups of poly(oxyalkylene) onto a high molecular weight polymer backbone, preferably by irradiation.
  • Figure 3 contains a graphical representation of the effect of copolymer composition on retention ability, determined by flocculation ability as described in the Examples below;
  • Figure 4 contains a graphical representation of the effect of polyethylene oxide chain length on retention ability, determined by flocculation ability as described in the Examples below;
  • Figure 5 contains a graphical representation of the effect of aging on retention ability, determined by flocculation ability as described in the Examples below;
  • Figure 6 contains a graphical representation of the effect of the composition of copolymer on retention ability, as determined by DDJ as described in the Examples below;
  • Figure 7 contains a graphical representation of the effect of PEO side chain length on retention ability, as determined by DDJ as described in the Examples below;
  • Figure 8 contains a graphical representation of the effect of shear on retention ability, as determined by DDJ as described in the Examples below;
  • Figure 9 contains a graphical representation of the retention ability of copolymers prepared by polymer-to- polymer grafting, as determined by flocculation ability, as described i .the Examples below.
  • the chemical retention aid provided herein employs a backbone polymer chain which is water soluble and of very high molecular weight onto which are provided many side chains of low molecular weight polyoxyethylene or other low molecular weight poly(oxyalkylene) so as to assist adhesion of the fines particles to the fibers during drainage of the pulp mat in sheet formation.
  • the backbone polymer chain has a molecular weight of at least about 100,000, generally in excess of about 500,000 and preferably at least about 3 million. In general, higher molecular weights lead to a higher efficiency of fines retention. The upper limit of molecular weight is largely determined by the ability to dissolve the polymer in the water.
  • the polyacrylamide backbone polymer chain is inexpensive to produce, is readily made and is much less sensitive to shear and metal ions than the high molecular weight polyethylene oxides conventionally employed, as may be seen in the experiments reported in the Examples below.
  • the polyacrylamide has a high molecular weight, generally at least about 100,000, as noted above.
  • the polyacrylamide polymer chain may be a homopolymer of acrylamide or lower alkylacrylamide, such as ethacrylamide or isopropylacrylamide, or a copolymer of two or more of such acrylamides.
  • the polymer chain generally is provided as a linear chain, but may comprise a branched chain or may be cross-linked.
  • the pendant groups generally comprise polyoxyethylene groups, although they may comprise polyoxypropylene groups, as well as copolymer mixtures or blocks of polyoxyethylene and polyoxypropylene.
  • the polyoxyalkyl groups may be provided pendant from the backbone polymer chain in any convenient manner.
  • One such procedure involves the copolymerization of acrylamide or other backbone monomer with an unsaturated macromonomer, usually a poly(oxyalkyl) substituted acrylate or methacrylate.
  • unsaturated macromonomer usually a poly(oxyalkyl) substituted acrylate or methacrylate.
  • unsaturated macromonomer may have the formula:
  • 0 C - [CH 2 CH 2 0] n -R where R and R' are independently -H or -CH 3 and n is the number of oxyethylene groups in each of the pendant chains, generally at least about 5.
  • Such polymerization may be effected by free-radical polymerization employing any convenient initiator.
  • the pendant low molecular weight polyethylene oxide side chains also may be provided by graft polymerization of poly(alkylene oxide) polymer onto the polyacrylamide backbone or backbone of other high molecular weight polymer.
  • a mixture of the low molecular weight polyethylene oxide generally one having the formula:
  • R, R' and R" are independently CH 3 or H and z is the number of pendant groups and is at least about 5, preferably at least about 10, and high molecular weight polyacrylamide, generally having a molecular weight of at least about 100,000, preferably at least about 500,000, more preferably at least about 1,000,000 and most preferably at least about 3,000,000, may be subjected to irradiation, such as by gamma radiation, to effect graft polymerization of the polyethylene oxide onto the backbone at random locations.
  • chemical grafting agents such as eerie ions or peroxides, may be employed with the mixture of polyethylene oxide and polyacrylamide.
  • the overall quantity of polyoxyethylene in the pendant side chains generally comprise at least about 0.1 mole % of the overall molecule and may vary up to a large value. However, it is usually preferred for the overall quantity of polyethylene to be about 0.15 to about 3 mole %.
  • the pendant poly(ethylene oxide) side chains provided in the copolymers utilized herein may still exhibit some sensitivity, the presence of a large number of much smaller chains decreases significantly the adverse effect of decomposition of polyoxyethylene in comparison to the conventional high molecular weight polyethylene material. This leads to the significant improvement in stability established by the copolymers used herein in comparison to the prior art high molecular weight polyethylene oxides, while achieving comparable efficiencies of fines retention.
  • a polymeric retention aid in accordance with the present invention may have a structure depicted as follows:
  • R, R' and R" are independently H or CH 3
  • x is the number of acrylamide monomer units in the length of the backbone chain, which is at least about 1400 (corresponding to a molecular weight of at least about 100,000), preferably at least corresponding to a molecular weight of about 3 x 10 6
  • z is the number of oxyethylene and/or oxypropylene groups in the side chain, wherein z is at least about 5, preferably about 5 to about 40.
  • novel retention aids are employed in conjunction with phenolic compounds, generally phenol-formaldehyde resins, as in the case of the conventionally employed high molecular weight polyoxyethylene polymers, in retaining fines in all forms of mechanical wood pulp.
  • This Example describes the preparation of graft copolymers by copolymerization of monomers.
  • copolymers were synthesized by copolymerization of acrylamide with a variety of polyoxyethylene macromonomers of the structure:
  • K ⁇ O g potassium persulfate
  • the compositions of the graft copolymers were measured by NMR and HPLC. Molecular weight of the graft copolymer was measured by GPC, light scattering and intrinsic viscosity.
  • This Example describes the experimental protocol for testing flocculation of polystyrene resin particles.
  • the graft copolymers prepared as described in Example 1, were used to test for the ability to cause monodisperse polystyrene latex particle to flocculate in the presence of wood fibers and phenol-formaldehyde resin, as a measure of the ability of the graft polymers to cause fines retention in wood pulps.
  • the polystyrene latex particles used in such tests were synthesized using emulsifier-free polymerization, employing 73 g styrene, 0.53 g of potassium sulfate in 670 g of distilled and deionized water. Polymerization was carried out at 70 ° C for 12 hours. The particle size of the polystyrene latex was measured using a BI-DCP particle sizer (Brookhaven Instrument Company) and is presented in the following Table I:
  • Flocculation of the latex was induced by the sequential addition of small quantities (1.0 to 4.0 mg/L) of graft copolymer or high molecular weight polyethylene oxide (Polyox 301, MWt. 4 million, Polyox 309, MWt. 8 million, Union Carbide Corporation, materials commercially used as retention aids) for comparison, and phenolic resin Cascophen C27, Borden) (40% aqueous solution) , in the presence of wood fiber.
  • small quantities 1.0 to 4.0 mg/L
  • phenolic resin Cascophen C27, Borden (40% aqueous solution)
  • aqueous solution of graft copolymer or polyethylene oxide then was added at a concentration of 0.025 to 0.05 wt.% to a total volume of 50 mL.
  • the samples were hand-shaken for 3 to 5 seconds and the suspended solids were allowed to settle for one hour at room temperature.
  • the supernatant then was taken from the tube and filtered through a 200 mesh screen to remove suspended fiber fragments and the turbidity was measured.
  • both Polyox 301 and 309 have an optimum addition of 2 mg/L and hence an optimum weight ratio of polyethylene oxide to phenolic resin of 1:1.
  • the flocculation efficiency initially increased with increasing amounts of copolymer, the copolymer concentrations yielding minimum relative turbidity values ranged between 2 and 4 mg/L.
  • higher copolymer concentrations > 4 mg/L caused flocculation to deteriorate.
  • the polyethylene oxides alone did not flocculate the latex to any significant degree, the copolymers alone were able to achieve about 25% latex removal, corresponding to a relative turbidity of 0.75. No flocculation was observed using polyacrylamide and phenol-formaldehyde resin.
  • This Example illustrates the effect of the composition of the copolymer on flocculation.
  • acrylamide at different ratios of monomers, one copoly erized at 25"C, another copolymerized at 40 * C, were tested for formulation performance following the procedure of Example 2. The results obtained are shown graphically in Figure 3.
  • This Example illustrates the effect of polyethylene oxide chain length in the copolymer on flocculation.
  • the copolymers in both cases contained about 0.7 to 0.8 % (mol) of macromonomer but had different chain lengths.
  • This Example illustrates the effect of molecular weight of copolymer on flocculation.
  • Example 7 This Example illustrates the effect of aging polymers in aqueous solution on flocculation.
  • the copolymer provided herein maintained its flocculation performance over various periods of aging, while the performance of both Polyol 301 and Polyol 309 declined steadily with an increasing storage period. After 20 days of storage, the Polyols had almost completely lost their ability to flocculate, while the copolymer sample retained its performance over the same period.
  • This copolymer had a molecular weight of 3.7 x 10° and contained 0.65 mole % of MA-23 macromonomer.
  • This Example describes evaluation of the copolymers by Dynamic Drainage Jar (DDJ) .
  • FPR for PEO homopolymers also showed a strong dependence on molecular weight. FPR increased to 83.7% for Polyox 309 with molecular weight of 8 million from 70% for Polyox 301 with a molecular weight of 4 million.
  • Figure 6 shows the influence of composition on amount of polyethylene oxide pendant chains on FPR measurements for copolymers prepared at 25'C and 40"C.
  • Figure 8 shows the effect of propeller speed of FPR of newsprint pulp, for copolymers provided herein and Polyox 309.
  • the results depicted in Figure 8 show the improved resistance to shear exhibited by the copolymers provided herein in comparison to Polyox 309.
  • a common trend was that FPR decreased as the propeller speed increased, but the decrease was more significant in the case of Polyox 309.
  • PEO low molecular weight polyethylene oxides
  • PAM high molecular weight polyacrylamide
  • Example 9 illustrates the flocculation ability of the graft copolymers prepared as described in Example 9.
  • the flocculation ability of the copolymers prepared in the preceding Example 9 was determined following the procedure described above in Example 2. The results obtained in comparison to PEO-309 are summarized in Figure 9.
  • the present invention provides a novel chemical retention aid for mechanical pulps which is inexpensive to manufacture, easy to make and exhibit chemical and physical stability not evident in prior art retention aids. Modifications are possible within the scope of this invention.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paper (AREA)

Abstract

On utilise des copolymères à haut poids moléculaire (c'est-à-dire d'au moins 100.000) ayant une ossature à base de polymère hydrosoluble (généralement un polyacrylamide) et des chaînes latérales de poly(oxyde d'alkylène), généralement de poly(oxyde d'éthylène), à raison de 0,15 % en moles environ à 3 % en moles environ, comme adjuvants de rétention lors de la formation de la feuille à partir de pulpe de bois (en particulier à partir de pulpe mécanique), en même temps que des composés phénoliques conventionnels, à la place des polymères poly(oxyde d'éthylène) à très haut poids moléculaire. Ces copolymères sont beaucoup moins sensibles à la dégradation et à la perte d'efficacité que les polymères poly(oxyde d'éthylène). Ces copolymères servant d'adjuvants de rétention peuvent être préparés par copolymérisation de monomères ou par greffage des chaînes du polymère poly(oxyde d'éthylène) sur l'ossature de polyacrylamide, à l'aide de radiations.
PCT/CA1994/000021 1993-01-19 1994-01-18 Adjuvants de retention pour les pates mecaniques Ceased WO1994017243A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP94904545A EP0680532A1 (fr) 1993-01-19 1994-01-18 Adjuvants de retention pour les pates mecaniques
JP6516508A JPH08504900A (ja) 1993-01-19 1994-01-18 機械パルプ用の歩留り向上剤
FI953468A FI953468L (fi) 1993-01-19 1994-01-18 Retentioaineet mekaanisia massoja varten

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9300939.7 1993-01-19
GB939300939A GB9300939D0 (en) 1993-01-19 1993-01-19 Retention aids for mechanical pulps

Publications (1)

Publication Number Publication Date
WO1994017243A1 true WO1994017243A1 (fr) 1994-08-04

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PCT/CA1994/000021 Ceased WO1994017243A1 (fr) 1993-01-19 1994-01-18 Adjuvants de retention pour les pates mecaniques

Country Status (6)

Country Link
EP (1) EP0680532A1 (fr)
JP (1) JPH08504900A (fr)
CA (1) CA2153997A1 (fr)
FI (1) FI953468L (fr)
GB (1) GB9300939D0 (fr)
WO (1) WO1994017243A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0773319A1 (fr) * 1995-11-08 1997-05-14 Nalco Chemical Company Méthode pour améliorer les performances des polymères et copolymères d'acrylamide utilisés en tant que floculants et agents de rétention
WO1999002775A1 (fr) * 1997-07-07 1999-01-21 Kemira Kemi Ab Agent de retention
US6033524A (en) * 1997-11-24 2000-03-07 Nalco Chemical Company Selective retention of filling components and improved control of sheet properties by enhancing additive pretreatment

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0980330A (ja) * 1995-09-07 1997-03-28 Minolta Co Ltd マルチビーム走査光学系

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2549089A1 (de) * 1974-11-15 1976-05-26 Sandoz Ag Retentions- und entwaesserungsmittel fuer papier
EP0203817A1 (fr) * 1985-05-31 1986-12-03 Betz Europe, Inc. Compositions polymères

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2549089A1 (de) * 1974-11-15 1976-05-26 Sandoz Ag Retentions- und entwaesserungsmittel fuer papier
EP0203817A1 (fr) * 1985-05-31 1986-12-03 Betz Europe, Inc. Compositions polymères

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0773319A1 (fr) * 1995-11-08 1997-05-14 Nalco Chemical Company Méthode pour améliorer les performances des polymères et copolymères d'acrylamide utilisés en tant que floculants et agents de rétention
US6048438A (en) * 1995-11-08 2000-04-11 Nalco Chemical Company Method to enhance the performance of polymers and copolymers of acrylamide as flocculants and retention aids
WO1999002775A1 (fr) * 1997-07-07 1999-01-21 Kemira Kemi Ab Agent de retention
US6306256B1 (en) 1997-07-07 2001-10-23 Kemira Kemi Ab Retention agent
US6033524A (en) * 1997-11-24 2000-03-07 Nalco Chemical Company Selective retention of filling components and improved control of sheet properties by enhancing additive pretreatment

Also Published As

Publication number Publication date
GB9300939D0 (en) 1993-03-10
EP0680532A1 (fr) 1995-11-08
FI953468A7 (fi) 1995-08-28
FI953468L (fi) 1995-08-28
CA2153997A1 (fr) 1994-08-04
FI953468A0 (fi) 1995-07-18
JPH08504900A (ja) 1996-05-28

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